CN109876493A - Thin-layer chromatography column and working method - Google Patents

Thin-layer chromatography column and working method Download PDF

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Publication number
CN109876493A
CN109876493A CN201910230010.7A CN201910230010A CN109876493A CN 109876493 A CN109876493 A CN 109876493A CN 201910230010 A CN201910230010 A CN 201910230010A CN 109876493 A CN109876493 A CN 109876493A
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Prior art keywords
cylinder
thin
cross
section
layer chromatography
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CN201910230010.7A
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Chinese (zh)
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马良
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Minjiang University
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Minjiang University
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Abstract

The present invention relates to a kind of thin-layer chromatography columns, cylinder including being in flat cylindrical, the cylinder have hollow inner cavity, and the top of the cylinder has opening, the lower part of the cylinder is provided with the outlet tube being connected with the inner cavity of cylinder, and the cock to open and close outlet tube is provided on the outlet tube;The invention further relates to a kind of working methods of thin-layer chromatography column.Not only structure design is simple, reasonable by the present invention, but also can effectively improve fixed phase stuffing distributing homogeneity in chromatographic column, improves separation and purification success rate, reduces dark color sample separation process operation difficulty.

Description

Thin-layer chromatography column and working method
Technical field
The present invention relates to a kind of thin-layer chromatography column and working methods.
Background technique
Column chromatography (chromatography) technology is commonly analysis and process for separation and purification in a kind of laboratory and industrial production, can be high Object or removal impurity is rapidly separated from the mixture in effect, is also commonly used for sample concentration, purification or solution replacement etc.. Chromatography is difference (such as molecular shape and size, Molecular Adsorption power, the distribution using each component physicochemical properties in mixture Coefficient etc.), keep each component different with the distributed degrees in mobile phase in stationary phase, each component is caused to move at different rates, It is finally reached the effect of separation, there are good separating effect, simple operation and other advantages.
Chromatographic column is usually the cylindrical type glass tube that a lower end has plug valve, has one layer of fixed sand in column bottom Core, centre are stationary phase (adsorbent) fillers, and most upper one layer repaves one layer of quartz sand.Dress column process is divided into wet method dress post and dry method Column is filled, it is that column chromatography success isolates and purifies one of committed step of substance that the quality of pillar dress is good and bad.Generally want It asks pillar to fill uniform, cannot be layered, cannot there is bubble etc. in pillar.After filling column, sample mixture is added, supplement is few Eluant, eluent is measured, plug valve is opened, makes under liquid flow.After observing that sample enters quartz sand layer by chromatographic column glass wall, It adds other eluant, eluents to be eluted, until colour band is unfolded.
When separating the deeper blend sample of some colors (such as dyestuff) using cylindrical type glass chromatography column, due in sample Impurity often with certain color, and the light transmittance of cylindrical type chromatographic column is relatively low, and a small amount of hangover will be observed Less than the expansion situation of colour band, the operation difficulty of chromatography process is increased.In addition, no matter wet process or dry column-packing process In, achieve the purpose that remove bubble frequently by the method for tapping chromatographic column and keeps adsorbent upper end horizontal.However, tapping The amount of force that filler is subject in chromatographic column in the process is inconsistent, and the stress close from glass wall is larger, it is remote from glass wall by Power is smaller, affects the uniformity of adsorbent distribution, and then influence the uniformity of flow velocity and colour band, causes chromatographic column effective Separation and purification.
Summary of the invention
In view of the deficiencies in the prior art, technical problem to be solved by the invention is to provide a kind of thin-layer chromatography column and work Method, it is not only reasonable in design but also efficiently convenient.
It in order to solve the above-mentioned technical problem, the technical scheme is that a kind of thin-layer chromatography column, including is in flat cylindrical Cylinder, the cylinder has hollow inner cavity, and the top of the cylinder has opening, and the lower part of the cylinder is provided with and column The outlet tube that the inner cavity of body is connected is provided with the cock to open and close outlet tube on the outlet tube.
Further, the cross section of the cylinder is in four frame shapes.
Further, the cross section of the cylinder is parallel four frame shape, the cross section of the cylinder by two interior long sides, Two outer long sides, two inner short-sides and two outer short sides surround, the distance between two interior long sides of the cross section of the cylinder For 0.1mm ~ 50mm.
Further, the cross section of the cylinder is four frame shape of curl, the cross section of the cylinder by two interior long sides, Two outer long sides, two inner short-sides and two outer short sides surround, two interior long sides of the cross section of the cylinder and two foreign ministers While being the curve of indent, the distance between two interior long sides of the cross section of the cylinder are 0.1mm ~ 50mm.
Further, two interior long sides of the cross section of the cylinder are arranged concentrically.
Further, the cylinder is made of glass, quartz or transparent polypropylene.
A kind of working method of thin-layer chromatography column includes following step including thin-layer chromatography column described in above-mentioned any one It is rapid: after mixing by eluant, eluent and fixed phase stuffing, the cylinder for having been loaded with part eluant, eluent to be injected into suction pipe or syringe It is interior, it opens cock and catches the eluant, eluent of outflow with container and constantly beat cylinder in the process, make the intracorporal stationary phase of column Filler starts uniformly to sink in eluant, eluent while soaked by uniform shock effect and exclude bubble;When in fixed phase stuffing Removal of bubbles is clean, and when the height of fixed phase stuffing is no longer changed, one layer of quartz is added in the top layer of fixed phase stuffing Sand adds sample after stablizing.
Compared with prior art, the invention has the following advantages: structure of the invention design is simple, reasonable, stationary phase Filler is filled in the four side cylindrical spaces an of thin layer, and fixed phase stuffing and chromatography being closer of post jamb, difference are smaller, is kept away It is inconsistent and lead to distribution different location filler is subject in cylindrical type chromatographic column during percussion amount of force has been exempted from Inhomogeneities.In addition, separating the deeper sample of some colors, since stationary phase is relatively thin, light transmittance is higher, so being easier to see The colour band expansion situation for examining sample, reduces the operation difficulty of chromatography process.
The present invention will be further described in detail with reference to the accompanying drawings and detailed description.
Detailed description of the invention
Fig. 1 is the organigram of the embodiment of the present invention one.
Fig. 2 is the construction schematic top plan view of the embodiment of the present invention one.
Fig. 3 is the organigram of the embodiment of the present invention two.
Fig. 4 is the construction schematic top plan view of the embodiment of the present invention two.
Fig. 5 is the use state diagram of the embodiment of the present invention.
Fig. 6 is the use state diagram of the embodiment of the present invention.
In figure: 1- cylinder, 2- outlet tube, 3- cock, 4- syringe, 5- fixed phase stuffing, the fixed sand core of 6-, 7- rubber Plug, 8- conical flask, 9- air-inlet of vacuum pump, 10- vacuum pump, 11- vacuum valve, 12- vacuum pump gas outlet, 13- vaccum pump motor.
Specific embodiment
To make the foregoing features and advantages of the present invention clearer and more comprehensible, special embodiment below, and cooperate attached drawing, make detailed Carefully it is described as follows.
As shown in Fig. 1 ~ 6, a kind of thin-layer chromatography column, the cylinder 1 including being in flat cylindrical, the cylinder 1 has hollow The top of inner cavity, the cylinder 1 has opening, and the lower part of the cylinder 1 is provided with the outlet tube being connected with the inner cavity of cylinder 1 2, the cock 3 to open and close outlet tube 2 is provided on the outlet tube 2.
In embodiments of the present invention, the cross section of the cylinder 1 is in four frame shapes.
In the embodiment of the present invention one, the cross section of the cylinder 1 is parallel four frame shape, the cross section of the cylinder 1 It is surrounded by two interior long sides, two outer long sides, two inner short-sides and two outer short sides, in two of the cross section of the cylinder 1 The distance between long side is 0.1mm ~ 50mm.
In the embodiment of the present invention one, the cross section of the cylinder 1 is four frame shape of curl, the cross section of the cylinder 1 It is surrounded by two interior long sides, two outer long sides, two inner short-sides and two outer short sides, in two of the cross section of the cylinder 1 Long side and two outer long sides are the curve of indent, and the distance between two interior long sides of cross section of the cylinder 1 are 0.1mm ~50mm。
In the embodiment of the present invention one, two interior long sides of the cross section of the cylinder 1 are arranged concentrically.
In embodiments of the present invention, the cylinder 1 is made of glass, quartz or transparent polypropylene.
A kind of working method of thin-layer chromatography column includes following step including thin-layer chromatography column described in above-mentioned any one It is rapid: after mixing by eluant, eluent and fixed phase stuffing 5, the column for having been loaded with part eluant, eluent to be injected into suction pipe or syringe 4 In body 1, opens cock 3 and catch the eluant, eluent of outflow with container and constantly beat cylinder 1 in the process, make in cylinder 1 Fixed phase stuffing 5 starts uniformly to sink in eluant, eluent while soaked by uniform shock effect and exclude bubble;Work as stationary phase Removal of bubbles in filler 5 is clean, when the height of fixed phase stuffing 5 is no longer changed, adds in the top layer of fixed phase stuffing 5 Enter one layer of quartz sand, sample is added after stablizing.
In the embodiment of the present invention one, the specific steps are as follows:
Step (1): selecting a thin-layer chromatography column, and the pillar height H of the cylinder 1 of thin-layer chromatography column is 300mm, the column of thin-layer chromatography column The interior edge lengths L of the cross section of body 1 is 150mm, and the interior hem width degree W of the cross section of the cylinder 1 of thin-layer chromatography column is 10mm, is washed dry Only, the eluant, eluent of 1/2 pillar height is initially charged with after drying;
Step (2): the silica gel for selecting 400 mesh dry is as fixed phase stuffing 5, by eluant, eluent and fixed phase stuffing 5 with 1.5:1 weight The eluant, eluent mixed and fixed phase stuffing 5 are poured into the inner cavity of cylinder 1 than being uniformly mixed by amount, are opened cock 3 and are connect with container The eluant, eluent firmly flowed out elutes remaining fixed phase stuffing 5 on the inner wall of cylinder 1 with the eluant, eluent under suction pipe suck stream, herein In the process, cylinder 1 is constantly beaten, fixed phase stuffing 5 excludes to start uniformly to sink in eluant, eluent while bubble;
Step (3): observing that fixed phase stuffing 5 is no longer entirely wetted from the side of thin-layer chromatography column and top, and removal of bubbles is clean, When the height of fixed phase stuffing 5 is no longer changed, adds the quartz sand of one layer of 0.5cm in the upper end of thin-layer chromatography column, use simultaneously Syringe 4 supplements eluant, eluent, and sample is added after stablizing.
In the embodiment of the present invention two, the specific steps are as follows:
Step (1): selecting a thin-layer chromatography column, and the pillar height H of the cylinder 1 of thin-layer chromatography column is 250mm, the column of thin-layer chromatography column The interior edge lengths L of the cross section of body 1 is 300mm, and the interior hem width degree W of the cross section of the cylinder 1 of thin-layer chromatography column is 3mm;
Step (2): the silica gel for selecting 800 mesh dry is as fixed phase stuffing 5, by eluant, eluent and fixed phase stuffing 5 with 2.5:1 weight Inner cavity of the amount than pouring into cylinder 1 after mixing sucks remaining fixation on the inner wall of eluant, eluent elution cylinder 1 with syringe 4 Phase filling 5 opens cock 3 and catches the eluant, eluent of outflow with container, starts vacuum pump 10, careful to open cock 3, in negative pressure item Under part, cylinder 1 is beaten, excludes bubble, the beginning of fixed phase stuffing 5 uniformly sinks in eluant, eluent;
Step (3): adding the quartz sand of one layer of 0.5cm in the upper end of thin-layer chromatography column, sample is added after stablizing, and observes sample Situation is unfolded in the colour band of product, and regulating cock 3 is accelerated the eluant, eluent flow velocity in the cylinder 1 of thin-layer chromatography column under condition of negative pressure, mentioned High sample separation expansion efficiency.
For indicating that the term of positional relationship or shape removes applied in any technical solution disclosed in aforementioned present invention Its otherwise indicated outer meaning includes approximate with its, similar or close state or shape.
Either component provided by the invention by multiple individual component parts either assembled, or one The separate part that forming technology manufactures.
The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof;Although referring to preferred embodiment pair The present invention is described in detail, it should be understood by those ordinary skilled in the art that: still can be to of the invention specific Embodiment is modified or some technical features can be equivalently replaced;Without departing from the spirit of the technical scheme of the invention, It should all cover within the scope of the technical scheme claimed by the invention.

Claims (7)

1. a kind of thin-layer chromatography column, it is characterised in that: the cylinder including being in flat cylindrical, the cylinder have hollow inner cavity, The top of the cylinder has opening, and the lower part of the cylinder is provided with the outlet tube being connected with the inner cavity of cylinder, it is described go out The cock to open and close outlet tube is provided in liquid pipe.
2. thin-layer chromatography column according to claim 1, it is characterised in that: the cross section of the cylinder is in four frame shapes.
3. thin-layer chromatography column according to claim 2, it is characterised in that: the cross section of the cylinder is parallel four frame The cross section of shape, the cylinder is surrounded by two interior long sides, two outer long sides, two inner short-sides and two outer short sides, the column The distance between two interior long sides of the cross section of body are 0.1mm ~ 50mm.
4. thin-layer chromatography column according to claim 2, it is characterised in that: the cross section of the cylinder is four frame of curl The cross section of shape, the cylinder is surrounded by two interior long sides, two outer long sides, two inner short-sides and two outer short sides, the column The two interior long sides and two outer long sides of the cross section of body are the curve of indent, two interior long sides of the cross section of the cylinder The distance between be 0.1mm ~ 50mm.
5. thin-layer chromatography column according to claim 4, it is characterised in that: two interior long sides of the cross section of the cylinder are same Heart setting.
6. thin-layer chromatography column according to claim 1, it is characterised in that: the cylinder is by glass, quartz or transparent poly- third Alkene is made.
7. a kind of working method of thin-layer chromatography column, which is characterized in that including the thin layer as described in claim 1 ~ 6 any one Chromatographic column comprising the steps of: after mixing by eluant, eluent and fixed phase stuffing, be injected into and had been loaded with suction pipe or syringe In the cylinder of part eluant, eluent, opens cock and catches the eluant, eluent of outflow with container and constantly beat cylinder in the process, The intracorporal fixed phase stuffing of column is set to start uniformly to sink in eluant, eluent while soaked by uniform shock effect and exclude bubble; When the removal of bubbles in fixed phase stuffing is clean, when the height of fixed phase stuffing is no longer changed, fixed phase stuffing most One layer of quartz sand is added in upper layer, and sample is added after stablizing.
CN201910230010.7A 2019-03-26 2019-03-26 Thin-layer chromatography column and working method Pending CN109876493A (en)

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CN201910230010.7A CN109876493A (en) 2019-03-26 2019-03-26 Thin-layer chromatography column and working method

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015083292A1 (en) * 2013-12-06 2015-06-11 株式会社日立製作所 Method and apparatus for separating rare earth ions
CN105505574A (en) * 2015-12-04 2016-04-20 南京威尔化工有限公司 Method for preparing high-purity ricinus oil according to chromatographic separation
KR20160059520A (en) * 2014-11-18 2016-05-27 인하대학교 산학협력단 Plate-type chromatographic device comprising chromatography column and holder
CN106442822A (en) * 2015-08-05 2017-02-22 无锡加莱克色谱科技有限公司 Homogenate tank filled with high performance liquid chromatographic column, filling device and filling method
CN106621461A (en) * 2016-12-13 2017-05-10 北京科技大学 Efficient separating device based on chromatographic theory

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015083292A1 (en) * 2013-12-06 2015-06-11 株式会社日立製作所 Method and apparatus for separating rare earth ions
KR20160059520A (en) * 2014-11-18 2016-05-27 인하대학교 산학협력단 Plate-type chromatographic device comprising chromatography column and holder
CN106442822A (en) * 2015-08-05 2017-02-22 无锡加莱克色谱科技有限公司 Homogenate tank filled with high performance liquid chromatographic column, filling device and filling method
CN105505574A (en) * 2015-12-04 2016-04-20 南京威尔化工有限公司 Method for preparing high-purity ricinus oil according to chromatographic separation
CN106621461A (en) * 2016-12-13 2017-05-10 北京科技大学 Efficient separating device based on chromatographic theory

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Application publication date: 20190614